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The structure of a new mineral jadarite, LiNaSiB3O7(OH) (IMA mineral 2006–36), has been determined by simulated annealing and Rietveld refinement of laboratory X-ray powder diffraction data. The structure contains a layer of corner-sharing, tetrahedrally coordinated Li, Si and B forming an unbranched vierer single layer, which is decorated with triangular BO3 groups. The Na ion is situated between the tetrahedral layers in a distorted octahedral site. As the very high boron content in this mineral makes obtaining neutron diffraction data very problematic, ab initio optimization using VASP was used to validate the structure and to better localize the H atom. The H atom is located on the apex of the triangular BO3 group and is involved in a weak intralayer hydrogen bond. The final Rietveld refinement agrees with the ab initio optimization with regard to a hydrogen bond between the H atom and one of the tetrahedral corner O atoms. The refined structure seems to be of a remarkably high quality given the complexity of the structure, the high proportion of very light elements and the fact that it was determined from relatively low-resolution laboratory data over a limited 2θ range (10–90° 2θ).

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S0108768107010130/lm5008sup1.cif
Contains datablocks phase, global, section_1, section_2

txt

Text file https://doi.org/10.1107/S0108768107010130/lm5008sup2.txt
Supplementary material

pdf

Portable Document Format (PDF) file https://doi.org/10.1107/S0108768107010130/lm5008sup3.pdf
Coordinate tables

Computing details top

Data reduction: Topas 4 beta (14/7/2006); program(s) used to solve structure: Topas 4 beta (14/7/2006); program(s) used to refine structure: Topas 4 beta (14/7/2006); molecular graphics: Diamond 3.1d; software used to prepare material for publication: Topas 4 beta (14/7/2006).

Figures top
[Figure 1]
[Figure 2]
[Figure 3]
[Figure 4]
[Figure 5]
[Figure 6]
(phase) top
Crystal data top
B3HO8Si·Na·LiV = 594.18 (2) Å3
Mr = 219.46Z = 4
Monoclinic, P21/cDx = 2.453 Mg m3
Dm = 2.453 Mg m3
Dm measured by Bermann balance
Hall symbol: -P 2ybcCu Kα radiation, λ = 1.5418 Å
a = 6.7620 (1) ŵ = 4.51 mm1
b = 13.8016 (3) ÅT = 298 K
c = 7.6878 (2) Å, white
β = 124.089 (1)° × × mm
Data collection top
Bruker D8 Advance
diffractometer
h = ??
Absorption correction: for a cylinder mounted on the ϕ axis
Debye-Scherrer correction
k = ??
Tmin = ?, Tmax = ?l = ??
Refinement top
Refinement on F21 constraint
Least-squares matrix: fullH atoms treated by a mixture of independent and constrained refinement
S = 1.27Unit
87 parameters(Δ/σ)max = 0.001
Crystal data top
B3HO8Si·Na·LiV = 594.18 (2) Å3
Mr = 219.46Z = 4
Monoclinic, P21/cCu Kα radiation
a = 6.7620 (1) ŵ = 4.51 mm1
b = 13.8016 (3) ÅT = 298 K
c = 7.6878 (2) Å × × mm
β = 124.089 (1)°
Data collection top
Bruker D8 Advance
diffractometer
Tmin = ?, Tmax = ?
Absorption correction: for a cylinder mounted on the ϕ axis
Debye-Scherrer correction
Refinement top
S = 1.27H atoms treated by a mixture of independent and constrained refinement
87 parameters
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Li10.462 (2)0.1995 (6)0.1383 (15)0.046 (3)*
Na10.9733 (3)0.99060 (10)0.7544 (3)0.0764
B10.2096 (17)0.1602 (8)0.6623 (18)0.091 (3)*
B20.6920 (14)0.3493 (6)0.4160 (15)0.054 (2)*
B30.5290 (10)0.5022 (4)0.7860 (9)0.0947
Si10.0378 (4)0.7539 (2)0.2048 (3)0.0584 (5)*
O10.8157 (7)0.7241 (3)0.9895 (6)0.0651 (14)*
O20.2673 (7)0.7818 (3)0.2102 (6)0.0663 (13)*
O30.9733 (6)0.8483 (3)0.2873 (7)0.0581 (14)*
O40.1150 (5)0.6584 (3)0.3491 (6)0.0542 (13)*
O50.7457 (8)0.5506 (3)0.8761 (9)0.0708 (15)*
O60.6846 (9)0.4560 (3)0.3520 (8)0.0570 (13)*
O70.5489 (7)0.6725 (3)0.6198 (6)0.0634 (12)*
O80.5299 (3)0.4051 (3)0.8362 (6)0.0733 (14)*
H10.699 (3)0.3993 (14)0.936 (3)0.0953 (19)*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Na10.091 (6)0.0657 (18)0.081 (2)0.01 (7)0.038 (2)0.0046 (19)
B30.046 (7)0.158 (10)0.098 (11)0.016 (7)0.043 (8)0.078 (8)
Geometric parameters (Å, º) top
Li1—O11.882 (11)B1—O51.602 (12)
Li1—O21.898 (10)B2—O21.479 (12)
Li1—O81.957 (11)B2—O71.522 (11)
Li1—O71.978 (14)B2—O41.528 (9)
Li1—O72.598 (13)B2—O61.544 (10)
Li1—H12.36 (2)B3—O61.352 (7)
Na1—O42.212 (4)B3—O51.391 (7)
Na1—O32.303 (5)B3—O81.394 (7)
Na1—O52.477 (6)Si1—O11.542 (4)
Na1—O62.561 (7)Si1—O21.577 (6)
Na1—H12.579 (17)Si1—O41.611 (5)
Na1—O62.624 (5)Si1—O31.613 (5)
Na1—O52.728 (8)H1—O80.960 (15)
B1—O11.395 (14)H1—O32.155 (14)
B1—O31.493 (16)H1—O52.20 (2)
B1—O71.561 (9)
O1—Li1—O2108.8 (6)O2—B2—O7109.3 (7)
O2—Li1—O7103.9 (5)O2—B2—O4112.4 (6)
O2—Li1—O8102.1 (5)O2—B2—O6112.2 (6)
O8—Li1—O7120.1 (5)O7—B2—O4108.6 (7)
O4—Na1—O3150.49 (17)O6—B3—O5123.3 (6)
O4—Na1—O592.43 (15)O6—B3—O8117.6 (5)
O4—Na1—O6115.57 (17)O5—B3—O8119.0 (5)
O3—Na1—O594.79 (16)O1—Si1—O2116.4 (3)
O3—Na1—O688.16 (17)O1—Si1—O4105.4 (2)
O1—B1—O3122.4 (9)O1—Si1—O3108.8 (3)
O1—B1—O7113.2 (8)O2—Si1—O4104.3 (3)
O1—B1—O5113.0 (7)O4—Si1—O3116.5 (3)
O3—B1—O7104.5 (8)O8—H1—O3157.2 (17)

Experimental details

Crystal data
Chemical formulaB3HO8Si·Na·Li
Mr219.46
Crystal system, space groupMonoclinic, P21/c
Temperature (K)298
a, b, c (Å)6.7620 (1), 13.8016 (3), 7.6878 (2)
β (°) 124.089 (1)
V3)594.18 (2)
Z4
Radiation typeCu Kα
µ (mm1)4.51
Crystal size (mm) × ×
Data collection
DiffractometerBruker D8 Advance
diffractometer
Absorption correctionFor a cylinder mounted on the ϕ axis
Debye-Scherrer correction
No. of measured, independent and
observed (?) reflections
?, ?, ?
Rint?
Refinement
R[F2 > 2σ(F2)], wR(F2), S ?, ?, 1.27
No. of reflections?
No. of parameters87
No. of restraints?
H-atom treatmentH atoms treated by a mixture of independent and constrained refinement
Δρmax, Δρmin (e Å3)?, ?

Computer programs: Topas 4 beta (14/7/2006), Diamond 3.1d.

 

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